KR100678501B1 - Seath-core polyester composite fiber having groove and manufacturing method thereof - Google Patents

Abstract

A sheath-core type polyester composite fiber having grooves and a manufacturing method thereof are provided to prevent the lowering of intensity of the fiber according to formation of the stripe pattern. A reformed polyester resin(10) and a regular polyester resin(20) are dried at 140 degrees in centigrade and supplied to the first extruder(1) and the second extruder(2), respectively. The first and second resins are melted and spun through a spinneret(3) at the temperature of 285-295 degrees in centigrade. Thereafter, the reformed polyester resin is positioned at a sheath portion and the regular polyester resin is positioned at a core portion so that a sheath-core type polyester composite fiber is manufactured. The fiber is wound by a winder(6) via the first godet roller(4) and the second godet roller(5).

Description

Groove-formed sheath-core fibrillated polyester composite fiber and its manufacturing method {SEATH-CORE POLYESTER COMPOSITE FIBER HAVING GROOVE AND MANUFACTURING METHOD THEREOF}

1 is a cross-sectional view of the sheath-core fibrillated polyester composite fiber in which the groove of the present invention is produced,

2 is an enlarged photograph 1000 times of the surface structure of the cis-core fibrillated polyester composite fiber in which the groove of the present invention is produced,

Fig. 3 is a schematic diagram of an apparatus for producing cis-core fibrillated polyester composite fibers in which grooves of the present invention are produced.

Description of Drawings

1: first extruder 2: second extruder

3: spinneret 4: first roller

5: second gourd roller 6: winder

10: modified polyester resin 20: regular polyester resin

The present invention relates to a fibrillated polyester composite fiber and a method of manufacturing the same, and more particularly, the fibrillated polyester composite fiber of the present invention is a sheath-core fibrillated polyester composite fiber, The present invention relates to a sheath-core fibrillated polyester composite fiber in which a groove is produced in which a polyester resin is used as a sheath part and a regular polyester resin is used as a core part.

In general, polyester resins having excellent physical and chemical properties are widely used as optical materials, industrial materials, and various clothing materials. However, in particular, polyester fibers used in clothing materials have the drawback that the surface is smooth, hard to the touch, and soft, because they are produced by melt spinning.

 Therefore, a conventional method for producing polyester fibers in the form of fine microfiber has been proposed as a conventional invention for solving the above drawbacks. As an example, Korean Patent Laid-Open Publication Nos. 2003-50001 and 2004-44800 disclose a composite spinning of a regular polyester resin and a modified polyester resin to prepare fibers, and then eluting the modified polyester resin to 0.5 denier or less. Disclosed is a method of making a fiber in the microfiprilated form of the same. However, although the inventions can obtain microfibers by eluting the modified polymer, there are disadvantages in that the manufacturing cost is increased and the manufacturing process is complicated due to the removal of the modified polymer. In addition, Korean Patent Laid-Open Publication No. 1999-17168 proposes a method for improving the surface feel by complex spinning of mutually incompatible polyamide and polyester resin. However, the fiber according to the present invention has a disadvantage in that it does not show uniform surface properties due to polyamide and polyester dyeing differences. In addition, Japanese Patent Application Laid-Open No. 9-170114 has copolymerized an organic sulfonic acid metal salt to a polyester polymer in order to improve dyeing properties and fibrillation properties, and specific fibrillation is generated by specific heat treatment and alkali reduction treatment so that the feel and dyeability Although excellent polyester fiber has been proposed, the organic sulfonic acid metal salt is copolymerized, and as a result, irregular gaps pass through the inside and the surface thereof, resulting in irregular fibrillation, causing a problem of lowering the strength of the fiber.

   Conventional inventions as described above have been directed to a method for controlling the microstructure of fibrillated fibers and improving the new texture and dyeability by fibrillation by a stable method, but the problem of lowering the strength of fibers due to excessive fibrillation There can be. In addition, the organic sulfonic acid salt as a modifier in the manufacturing process of the modified polyester resin is bubbled at a high temperature, there is a lot of difficulties in the manufacturing process according to the inclusion of the problem that the monomer is floating. Therefore, there is a need for a new method of improving such a floating phenomenon and strength.

Accordingly, the present inventors have tried to solve the conventional problems, as a result of the addition of an alkyl sulfonic acid metal salt that can form a groove in the polycondensation step of the polyester, and the alkyl sulfonic acid metal salt used to generate a bubble at a high temperature monomer In order to solve the problem in which the phenomenon of flotation occurs, the antifoaming agent is added in the polycondensation step, and in order to prevent the decrease in strength of the fiber due to the formation of streaks on the surface of the fabric, regular polyester and modified polyester are used. The present invention was completed by preparing the sheath-core composite fiber.

SUMMARY OF THE INVENTION An object of the present invention is to provide a sheath-core fibrillated polyester composite fiber and a method of manufacturing the same, in which groove strength is maintained and fiber strength is maintained, and monomer floating phenomenon is improved when the polyester resin is modified.

In order to achieve the above object, the present invention is 0.5 to 5.0 parts by weight of an alkyl sulfonic acid metal salt and an antifoaming agent with respect to 100 parts by weight of a polyester resin made of at least one kind of aromatic dicarboxylic acid and at least one kind of diol. To 0.05 part by weight before the esterification reaction or the polycondensation reaction to modify the polyester resin as the sheath portion, and the regular polyester resin as the core portion, the ratio of the sheath portion to the core portion is 40 to 60% by weight To provide a cis-core fibrillated polyester composite fiber in which the multispun grooves are produced.

The alkyl sulfonic acid metal salt is a compound represented by the following formula (1).

(Wherein, R ¹ is an alkyl group having 5 to 20 carbon atoms, M ¹ represents an alkali metal.)

 The alkyl sulfonic acid metal salt is preferably an alkyl sulfonic acid sodium salt, and the content of sodium is 500 to 6,000 ppm. In addition, the average molecular weight of the alkyl sulfonic acid metal salt is preferably 180 to 500, and the antifoaming agent uses a silicone-based antifoaming agent.

The polyester composite fiber has a width of 0.1 to 1 μm, a length of 10 to 40 μm, a depth of 0.1 to 1.5 μm, and fine stripe-shaped grooves are formed in the axial direction of the fiber.

In addition, the present invention 1) 0.5 to 5.0 parts by weight of an alkyl sulfonic acid metal salt and 0.001 to 0.05 part by weight of an antifoaming agent with respect to 100 parts by weight of a polyester resin composed of at least one kind of aromatic dicarboxylic acid and at least one kind of diol. Before the reaction or the polycondensation reaction to prepare a modified polyester resin,

2) The modified polyester resin prepared as the sheath portion, and the regular polyester resin as the core portion, the spinning ratio of the sheath portion to the core portion is 40 to 60% by weight of the composite spinning, the sheath-core form Preparing a composite fiber, and

3) after weaving the sheath-core composite fiber prepared above, a process for producing a groove-made sheath-core fibrillated polyester composite fiber, which comprises a step of reducing 10% to 30% in an alkaline solution to provide.

In step 1), the reaction temperature is carried out below 250 ℃.

The alkyl sulfonic acid metal salt is to use a compound represented by the following formula (1).

Formula 1

(Wherein, R ¹ is an alkyl group having 5 to 20 carbon atoms, M ¹ represents an alkali metal.)

Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.

Fig. 1 is a cross-sectional view of the sheath-core fibrillated polyester composite fiber in which the groove of the present invention is produced, wherein the modified polyester resin 10 is used as the sheath and the regular polyester resin 20 is used as the core. .

Specifically, the cis portion esterifies 0.5 to 5.0 parts by weight of an alkyl sulfonic acid metal salt and 0.001 to 0.05 parts by weight of an antifoaming agent with respect to 100 parts by weight of a polyester resin made of at least one kind of aromatic dicarboxylic acid and at least one kind of diol. It consists of a polyester resin which was added and modified before reaction or a polycondensation reaction.

The grooved cis-core fibrillated polyester composite fiber of the present invention uses a polyester resin modified by adding an alkyl sulfonic acid metal salt and an antifoaming agent as a modifier capable of forming grooves in the polycondensation step of the polyester. The problem is that the organic sulfonic acid salt added in the conventional polyester resin manufacturing process is bubbled at a high temperature and the monomers are floated. In addition, the present invention is to produce a fibrillated polyester composite fiber in the sheath-core form by using the modified polyester resin (10) as a sheath portion and the regular polyester resin (20) as a core portion, thereby forming a streak on the surface of the fiber It is possible to prevent the problem of reduced fiber strength.

As the alkyl sulfonic acid metal salt used in the present invention, it is preferable to use a compound represented by the following formula (1).

Formula 1

(Wherein, R ¹ is an alkyl group having 5 to 20 carbon atoms, M ¹ represents an alkali metal.)

The alkyl sulfonic acid metal salts form grooves in the polyester polycondensation step, preferably using alkyl sulfonic acid sodium salts. The sodium content in the sodium salt of alkyl sulfonate is 500 ~ 6,000ppm, and those free of impurities are used.

At this time, if the sodium content is less than 500 ppm, it is not preferable because the carbon number of the sodium salt of alkyl sulfonate is 5 or less, and if it is more than 6,000 ppm, it is not preferable because the carbon number becomes 20 or more.

In addition, the average molecular weight of the sodium alkyl sulfonate salt is preferably 180 to 500, wherein if the average molecular weight of the sodium alkyl sulfonate salt is less than 180, the problem with the ethylene glycol in the vacuum state of the polymerization reaction occurs is not preferred And, if it exceeds 500, it is not preferable due to the problem that the surface grooves are not generated because the alkyl sulfonic acid sodium salt is not removed in the alkali reduction process of the fiber produced.

The antifoaming agent is to prevent the alkyl sulfonic acid metal salt from forming bubbles at a high temperature, thereby preventing the monomer from floating. In the present invention, the antifoaming agent is added before the polycondensation reaction vacuum setting, the polycondensation reaction temperature is controlled to 250 ° C or less, more preferably 220 ° C to 250 ° C. At this time, if the reaction temperature is less than 220 ℃ it is not preferable to rapidly add a temperature for the polymerization reaction, if it exceeds 250 ℃, the problem that the alkyl sulfonic acid metal salt is floating is not preferable.

The antifoaming agent is characterized in that it is incompatible with the polyester resins (10,20), positive in permeability and diffusibility, and preferably, a silicone-based antifoaming agent having excellent thermal stability is used. The antifoaming agent used in the present invention can be selected and used synthetically or commercially.

The antifoaming agent used in the present invention is prepared by adding 0.001 to 0.05 parts by weight of antifoaming agent, more preferably 0.005 to 0.02 parts by weight based on 100 parts by weight of polyester resin to prepare a polyester resin having an intrinsic viscosity of 0.6 to 0.8 dl / g. .

At this time, if the antifoaming agent used is less than 0.001 parts by weight, it is not preferable because of the problem that does not act as an antifoaming agent, if it exceeds 0.05 parts by weight, it is preferable because of the problem of causing yellowing of the polyester and the problem of long reaction time Not.

The spinning ratio of the sheath to the core is 40 to 60% by weight of the composite spinning.

Accordingly, the sheath-core fibrillated composite fiber of the present invention has a width of 0.1 to 1 μm, a length of 10 to 40 μm, and a depth of 0.1 to 1.5 μm on the surface of the fiber, and has fine stripe-shaped grooves in the axial direction of the fiber. Is generated (Fig. 2).

More specifically, the step of preparing the cis-core fibrillated composite fiber of the present invention comprises the steps of preparing the modified polyester resin 10, step 2 of preparing the cis-core composite fiber, and reducing the composite fiber in an alkaline solution. Processing is made in step 3.

Fig. 3 is a schematic diagram of an apparatus for manufacturing a cis-core fibrillated polyester composite fiber in which grooves of the present invention are produced, wherein a modified polyester resin 10 and a regular polyester resin 20 are dried at 140 ° C. to obtain a first It is respectively supplied to the extruder 1 and the 2nd extruder 2, and melt-spun at the temperature of 285 degreeC-295 degreeC through the spinneret 3, and the modified polyester resin 10 is carried out in a sheath and a regular polyester resin (20) is made of a cis-core fibrillated polyester composite fiber placed in the core portion. Thereafter, after passing through the first roller roller 4 and the second roller roller 5, the winder 6 is wound up.

Step 1 is an esterification reaction or polycondensation reaction process, to prepare a modified polyester resin (10). The characteristics and amount of the alkyl sulfonic acid metal salt and the antifoaming agent are the same as those described for the cis-core fibrillated polyester composite fiber in which the groove is formed. In addition, the alkyl sulfonic acid metal salt is prepared in a slurry mixed state of 40% to 60% in at least one or more types of diols, more preferably at 50%.

In step 2, the spinning ratio of the sheath portion to the core portion is preferably 40 to 60% by weight of the composite spinning.

Subsequently, step 3 is a 10% to 30% weight loss treatment of the polyester composite fiber prepared from the step in an alkaline solution, preferably 25% or less. In addition, it is preferable that the alkali weight loss treatment produces a fine stripe-shaped groove having a width of 0.1 to 1 μm, a length of 10 to 40 μm, and a depth of 0.1 to 1.5 μm in the axial direction of the surface of the composite fiber.

Through the following examples will be described the present invention in detail. This embodiment is intended to describe in detail using the most preferred embodiment of the present invention to the extent that those skilled in the art can easily carry out the technical idea of the present invention, The range is not limited to these examples.

Example 1

In order to obtain 100 weight part of polyester resins, 86.5 weight part of terephthalic acid and 48.5 weight part of ethylene glycol were pressurized in the ester reactor, and it heated up from 200 degreeC to 250 degreeC. And, the esterification reaction while removing the effluent produced in the reactor. After the completion of the esterification reaction, the temperature of the polycondensation reaction tube was controlled to 250 ° C. or lower, and 0.015 parts by weight of a phosphoric acid compound and antimony trioxide were added to bishydroxyethyl terephthalate (BHET) in an oligomer state obtained in the esterification reaction. Part by weight and 0.01 part by weight of cobalt acetate were added, 1.0 part by weight of an alkyl sulfonic acid sodium salt slurried with ethylene glycol and having an average molecular weight of 180 to 500 was added, and an antifoaming agent (Toshiba Silicone Co., Ltd., product name TSF-433) 0.005 weight Part was added, stirred for 5 minutes, and sufficiently dispersed in bishydroxyethyl terephthalate (BHET).

And the said polycondensation reaction tube was depressurized, the vacuum degree was 1.0 torr or less, the temperature was raised to 285 degreeC, and reaction was advanced, and the polyester resin of the intrinsic viscosity was 0.65 dl / g. The polyester resin was chipped and dried at regular intervals while being solidified using cold water to prepare a modified polyester resin of the present invention. The modified polyester resin and the regular polyester resin obtained in the above process were spun using different melt extruders in order to use the sheath-core detention in the temperature range of 285 ° C to 295 ° C. After the yarn prepared through the above process was chopped, a weight loss treatment was performed in an alkaline solution to obtain a knit fabric having a weight loss of 25%.

Example 2

    It carried out similarly to Example 1 except adding 2.0 weight part of alkyl sulfonic acid sodium salts.

Example 3

   It carried out similarly to Example 1 except adding 4.0 weight part of alkyl sulfonate sodium salts, and 0.01 weight part of antifoamers.

Comparative Example 1

  The same procedure as in Example 1 was conducted except that the antifoaming agent was not added.

Comparative Example 2

    The same procedure as in Example 2 was conducted except that the antifoaming agent was not added.

The following Examples 1 to 3, Comparative Example 1 and Comparative Example 2 are shown in Table 1 by performing a physical property test by the following method.

(1) Floating phenomenon

Floating phenomena generated during the manufacturing process of the cis-core fibrillated polyester composite fiber were visually distinguished.

X: No floating and reaction takes place.

(Triangle | delta): There is no floating but reaction is unstable.

(Circle): Floating occurs and reaction does not occur.

  (2) ultimate viscosity

The cis-core fibrillated polyester composite fiber is dissolved in a phenol solvent and is a value measured using a Uberod viscometer.

  (3) mineral analysis

The alkyl sulfonic acid metal salt content of the cis-core fibrillated polyester composite fiber is a value obtained by dissolving the sample in a strong acid solvent using ICP (Inductively Coupled Plasma), and then removing the organic material.

  (4) surface observation

The knitted fabric of the finally obtained cis-core fibrillated polyester composite fiber was photographed at a magnification of 1,000 times with a scanning electron microscope, and visually distinguished.

G: The groove of a surface is clear.

B: Grooves on the surface are not clear and are entangled.

Referring to Table 1, Examples 1 to 3 were prepared by adding an antifoaming agent at the same time as the alkyl sulfonic acid metal salt during the polycondensation reaction, there was no floating phenomenon of the monomer, the desired ultimate viscosity of 0.6 to 0.8 dl / g The polyester resin of was able to be manufactured. In addition, the composite fibers produced in Examples 1 to 3 had clear grooves on the surface as shown in FIG. On the other hand, Comparative Examples 1 and 2 were prepared without the addition of an antifoaming agent, so that the flocculation phenomenon of the monomers occurred, so that the polyester resin having the desired intrinsic viscosity could not be produced, and thus the grooves of the surface of the composite fiber were clear. It was not possible to check the phenomenon of tangling.

The cis-core fibrillated polyester composite fiber of the present invention configured as described above has no monomer floating phenomenon and is excellent in intrinsic viscosity and surface properties.

The method for producing the cis-core fibrillated polyester composite fiber of the present invention has the effect of increasing the strength of the fiber by placing the regular polyester resin in the core.

Although the present invention has been described in detail only with respect to the described embodiments, it will be apparent to those skilled in the art that various modifications and variations are possible within the technical scope of the present invention, and such modifications and modifications belong to the appended claims.

Claims (9)

1) 0.5 to 5.0 parts by weight of an alkyl sulfonic acid metal salt and 0.001 to 0.05 parts by weight of an antifoaming agent with respect to 100 parts by weight of a polyester resin made of at least one kind of aromatic dicarboxylic acid and at least one kind of diol, or an esterification reaction or a polycondensation Before the reaction, the modified polyester resin was introduced into a cis part, 2) A sheath-core fibrillated polyester composite fiber in which grooves are produced, characterized in that a regular polyester resin is used as a core part, and the spinning ratio of the sheath part to the core part is 40 to 60% by weight. . The method of claim 1, The cis-core fibrillated polyester composite fiber, wherein the groove is produced, wherein the alkyl sulfonic acid metal salt is a compound represented by the following Chemical Formula 1. Formula 1

(Wherein, R ¹ is an alkyl group having 5 to 20 carbon atoms, M ¹ represents an alkali metal.) The method of claim 1,  And the alkyl sulfonic acid metal salt is an alkyl sulfonic acid sodium salt, and the content of sodium is 500 to 6,000 ppm. The groove-produced cis-core fibrillated polyester composite fiber. The method of claim 1, The groove is produced cis-core fibrillated polyester composite fiber, characterized in that the average molecular weight of the alkyl sulfonic acid metal salt is 180 to 500. The method of claim 1, The groove-made cis-core fibrillated polyester composite fiber, wherein the antifoaming agent is a silicone antifoaming agent. The method of claim 1, The polyester composite fiber has a width of 0.1 ~ 1㎛, a length of 10 ~ 40㎛, a depth of 0.1 ~ 1.5㎛ on the fiber surface, the fine stripe-shaped grooves are produced in the axial direction of the fiber Sheath-cored fibrillated polyester composite fiber with grooves formed. 1) 0.5 to 5.0 parts by weight of an alkyl sulfonic acid metal salt and 0.001 to 0.05 parts by weight of an antifoaming agent with respect to 100 parts by weight of a polyester resin composed of at least one type of aromatic dicarboxylic acid and at least one type of diol; Step 1 to prepare a modified polyester resin, 2) The modified polyester resin prepared as the sheath portion, and a regular polyester resin as the core portion, the spinning ratio of the sheath portion to the core portion is 40% to 60% by weight of the composite spinning, sheath-core composite Preparing a fiber; And 3) weaving the prepared composite fiber and then reducing the amount by 10% to 30% in an alkaline solution; The method of producing a cis-core fibrillated polyester composite fiber, wherein the groove of claim 1 is formed. The method of claim 7, wherein In the step 1, the reaction temperature is 220 ℃ ~ 250 ℃ characterized in that the grooves produced cis-core fibrillated polyester composite fiber manufacturing method. The method of claim 7, wherein The alkyl sulfonic acid metal salt is a compound represented by the following formula (1) characterized in that the grooves produced cis-core fibrillated polyester composite fiber manufacturing method. Formula 1

(Wherein, R ¹ is an alkyl group having 5 to 20 carbon atoms, M ¹ represents an alkali metal.)

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